JP2021527611A - カーボンナノチューブ、その製造方法およびこれを含む一次電池用の正極 - Google Patents
カーボンナノチューブ、その製造方法およびこれを含む一次電池用の正極 Download PDFInfo
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- JP2021527611A JP2021527611A JP2020567872A JP2020567872A JP2021527611A JP 2021527611 A JP2021527611 A JP 2021527611A JP 2020567872 A JP2020567872 A JP 2020567872A JP 2020567872 A JP2020567872 A JP 2020567872A JP 2021527611 A JP2021527611 A JP 2021527611A
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- carbon nanotubes
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Abstract
Description
R(Ω)=U/I
U(V):電位差(potential difference)
I(A):電流
RCF:補正係数
本発明の一実施形態によるカーボンナノチューブは、気孔容積が0.94cm3/g以上であり、絡み合い状である。
本発明の他の一実施形態によるカーボンナノチューブの製造方法は、1)主触媒前駆体および助触媒前駆体を含む混合物をγ‐Al2O3に担持し、活性担持体を製造するステップと、2)真空乾燥を含む多段乾燥により、前記活性担持体を乾燥するステップと、3)前記乾燥した活性担持体に熱処理を施し、担持触媒を製造するステップと、4)前記担持触媒の存在下で、カーボンナノチューブを製造するステップとを含む。
まず、主触媒前駆体および助触媒前駆体を含む混合物をγ‐Al2O3に担持し、活性担持体を製造する。
次いで、真空乾燥が含まれた多段乾燥により、前記活性担持体を乾燥する。
次いで、前記乾燥した活性担持体に熱処理を施し、担持触媒を製造する。
次いで、前記担持触媒の存在下で、カーボンナノチューブを製造する。
本発明のさらに他の一実施形態による一次電池用の正極は、気孔容積が0.94cm3/g以上であり、絡み合い状のカーボンナノチューブを含む正極活物質および結着剤を含む。
本発明の一次電池は、上述の一次電池用の正極を含み、負極、電解液をさらに含む。
1)カーボンナノチューブの製造
実施例1‐1
<担持触媒の製造>
主触媒前駆体としてCo(NO3)2・6H2O25.68g(Co:約88.2mmol)、助触媒前駆体としてNH4VO31.23g(V:約10.5mmol)、(NH4)6Mo7O24・4H2O0.76g(Mo:約4.3mmol)、クエン酸0.61gおよび蒸留水60mlを投入し、触媒前駆体溶液を製造した。前記触媒前駆体溶液の全量をγ‐Al2O3(商品名:SCCa5/200、製造社:Sasol)20g(約196.15mmol)に担持し、活性担持体を製造した。前記活性担持体を80℃の恒温槽で30分間撹拌し、熟成された活性担持体を製造した。
取得した担持触媒1gを流動層反応装置内に位置する内径が55mmである石英管の下部に装着した。流動層反応装置の内部を窒素雰囲気で690℃に一定な速度で昇温させた後、維持し、窒素ガスと水素、エチレンガスを2:0.5:1の体積比で2l/分で流しながら60分間合成し、カーボンナノチューブ(23.3g)を製造した。
主触媒前駆体としてCo(NO3)2・6H2O25.68g(Co:約88.2mmol)、助触媒前駆体としてNH4VO30.79g(V:約6.8mmol)および(NH4)6Mo7O24・4H2O1.14g(Mo:約6.5mmol)、クエン酸0.58gおよび蒸留水60mlを投入して触媒前駆体溶液を製造した以外は、実施例1と同じ方法で担持触媒、カーボンナノチューブ(19.1g)を製造した。
主触媒前駆体としてCo(NO3)2・6H2O25.68g(Co:約88mmol)、助触媒前駆体としてNH4VO30.89g(V:約7.6mmol)および(NH4)6Mo7O24・4H2O0.38g(Mo:2.2mmol)、クエン酸0.38gおよび蒸留水60mlを投入して触媒前駆体溶液を製造した以外は、実施例1と同じ方法で担持触媒、カーボンナノチューブ(20.4g)を製造した。
主触媒前駆体としてCo(NO3)2・6H2O25.68g(Co:約88.2mmol)、助触媒前駆体としてNH4VO31.75g(V:約15mmol)および(NH4)6Mo7O24・4H2O0.76g(Mo:約4.3mmol)、クエン酸0.76gおよび蒸留水60mlを投入して触媒前駆体溶液を製造した以外は、実施例1と同じ方法で担持触媒、カーボンナノチューブ(28g)を製造した。
主触媒前駆体としてCo(NO3)2・6H2O29.30g(Co:約100.7mmol)、助触媒前駆体としてNH4VO30.6g(V:約5.1mmol)および(NH4)6Mo7O24・4H2O0.95g(Mo:約5.4mmol)、クエン酸0.45gおよび蒸留水60mlを投入して触媒前駆体溶液を製造した以外は、実施例1と同じ方法で担持触媒、カーボンナノチューブ(18g)を製造した。
熟成された活性担持体を120℃、60分間1次常圧乾燥し、1次常圧乾燥した活性担持体を200℃、50mbarで60分間2次真空乾燥した以外は、実施例1と同じ方法で担持触媒、カーボンナノチューブ(14g)を製造した。
<担持触媒の製造>
主触媒前駆体としてCo(NO3)2・6H2O29.63g(Co:約101.9mmol)、助触媒前駆体としてNH4VO32.38g(V:約20.3mmol)、クエン酸1.19gおよび蒸留水80mlを投入し、触媒前駆体溶液を製造した。前記触媒前駆体溶液の全量をγ‐Al2O3(商品名:SCCa5/200、製造社:Sasol)20g(約196.15mmol)に担持し、活性担持体を製造した。前記活性担持体を80℃の恒温槽で30分間撹拌しながら熟成させた。
取得した担持触媒1gを流動層反応装置内に位置する内径が55mmである石英管の下部に装着した。流動層反応装置の内部を窒素雰囲気で690℃に一定な速度で昇温させた後、維持し、窒素ガスと水素、エチレンガスを2:0.5:1の体積比で2l/分で流しながら60分間合成し、カーボンナノチューブ(27.0g)を製造した。
熟成された活性担持体を120℃で240分間1次常圧乾燥し、前記1次常圧乾燥した活性担持体を200℃で360分間2次常圧乾燥した以外は、実施例1と同じ方法で担持触媒およびカーボンナノチューブ(21.6g)を製造した。
熟成された活性担持体を175℃、10mbarで1時間1次真空乾燥し、2次真空乾燥をしなかった以外は、実施例1と同じ方法で担持触媒およびカーボンナノチューブ(20g)を製造した。
熟成された活性担持体を120℃、150mbarで120分間1次真空乾燥し、2次真空乾燥をしなかった以外は、実施例1と同じ方法で担持触媒およびカーボンナノチューブ(21.3g)を製造した。
束型カーボンナノチューブ(商品名:BT1001M、製造社:LG Chem)を用いた。
前記製造されたカーボンナノチューブを下記項目に対して評価を行い、その結果を下記表2に示した。
R(Ω)=U/I
U(V):電位差(potential difference)
I(A):電流
RCF:補正係数
1)粉砕されたカーボンナノチューブおよび一次電池(リチウム‐硫黄電池)の製造
実施例2‐1〜2‐6
下記条件で実施例1‐1〜1‐6のカーボンナノチューブに対してボールミル工程を行って粉砕した。
ボール直径、3mm、
ボール重量:1kg、
ボール回転速度:230rpm、
ボールミル時間:15分
カーボンナノチューブ投入量:60g
容器:2L PE bottle
下記条件で、実施例1‐7のカーボンナノチューブに対してボールミル工程を行って粉砕した。
ボール直径:3mm
ボール重量:1kg
ボール回転速度:230rpm
ボールミル時間:5分
カーボンナノチューブ投入量:60g
容器:2L PE bottle
下記条件で、実施例1‐7のカーボンナノチューブに対してボールミル工程を行って粉砕した。
ボール直径:3mm
ボール重量:1kg
ボール回転速度:230rpm、
ボールミル時間:15分
カーボンナノチューブ投入量:60g
容器:2L PE bottle
比較例1‐1〜1‐4のカーボンナノチューブを用いて、前記実施例2‐1と同じ方法で粉砕されたカーボンナノチューブおよび一次電池を製造した。
実験例2‐1:粉砕されたカーボンナノチューブおよび一次電池(リチウム‐硫黄電池)の物性評価
実施例2‐1〜2‐8および比較例2‐1〜2‐4で粉砕されたカーボンナノチューブの物性を、前記実験例1‐1に記載の評価方法に基づいて評価し、一次電池としてリチウム‐硫黄電池に対しては、下記条件で初期放電容量を測定し、その結果を下記表3に示した。
1)正極および一次電池(リチウム‐塩化チオニル電池)の製造
実施例3‐1〜実施例3‐7、比較例3‐1および比較例3‐2
<正極の製造>
正極活物質、結着剤および溶媒などの正極組成物の成分および含量を、下記表4に示したように適用し、混合および撹拌により正極組成物を製造した。製造された正極組成物をエキスパンドニッケル(expanded nickel)基板上に有するようにコーティングした後、120℃および100mbarで240分間真空乾燥し、0.8mmの厚さを有する正極を製造した。
正極として実施例および比較例の正極、負極としてリチウム金属薄膜、電解液としてLiAlCl4塩をSOCl2溶媒に溶解した溶液(1.25M)を用いて、巻回型の電池を製造した。
(A‐2)実施例2‐8の粉砕されたカーボンナノチューブ
(A‐3)アセチレンブラック(AB):Denka社のSB50L
(A‐4)ケッチェンブラック(KB):LION社のEC3001J
(B)DAIKIN社のPTFE‐D(ポリテトラフルオロエチレン、PTFE)
(C‐1)イソプロピルアルコール(IPA)
(C‐2)水
実験例3‐1
実施例および比較例の正極組成物、正極および一次電池の物性を下記の方法で測定し、その結果を下記の[表5]に記載した。
×:クラック未発生、○:クラック発生
Claims (19)
- 気孔容積が0.94cm3/g以上であり、絡み合い状である、カーボンナノチューブ。
- 気孔容積が0.95cm3/g以上である、請求項1に記載のカーボンナノチューブ。
- 25℃の温度および20kNの圧力で体積抵抗率が0.0187Ω・cm以下である、請求項1または2に記載のカーボンナノチューブ。
- 比表面積が200〜300m2/gである、請求項1から3のいずれか一項に記載のカーボンナノチューブ。
- 主触媒前駆体および助触媒前駆体を含む混合物をγ‐Al2O3に担持し、活性担持体を製造するステップと、
真空乾燥を含む多段乾燥により、前記活性担持体を乾燥するステップと、
前記乾燥した活性担持体に熱処理を施し、担持触媒を製造するステップと、
前記担持触媒の存在下で、カーボンナノチューブを製造するステップとを含む、カーボンナノチューブの製造方法。 - 前記多段乾燥は、常圧乾燥と、真空乾燥とを含む、請求項5に記載のカーボンナノチューブの製造方法。
- 前記常圧乾燥は、80〜160℃で行われる、請求項6に記載のカーボンナノチューブの製造方法。
- 前記真空乾燥は、80〜300℃の温度、および1〜200mbarの圧力で行われる、請求項6または7に記載のカーボンナノチューブの製造方法。
- 前記多段乾燥は、第1温度で行われる1次真空乾燥と、前記第1温度よりも高い第2温度で行われる2次真空乾燥とを含む、請求項5に記載のカーボンナノチューブの製造方法。
- 前記第1温度は80〜160℃であり、前記第2温度は175〜300℃である、請求項9に記載のカーボンナノチューブの製造方法。
- 前記助触媒は、バナジウムおよびモリブデンからなる群から選択される1種以上である、請求項5から10のいずれか一項に記載のカーボンナノチューブの製造方法。
- 前記混合物は、バナジウムおよびモリブデンの和とバナジウムのモル比が1:0.45〜1:0.95になるように助触媒前駆体を含む、請求項5から11のいずれか一項に記載のカーボンナノチューブの製造方法。
- 気孔容積が0.94cm3/g以上であり、絡み合い状であるカーボンナノチューブを含む正極活物質と、
結着剤とを含む、一次電池用の正極。 - 気孔容積が0.25cm3/g以上であり、平均気孔径が13.5nm以上である、請求項13に記載の一次電池用の正極。
- 比表面積が60〜200m2/gである、請求項13または14に記載の一次電池用の正極。
- 前記カーボンナノチューブは、気孔容積が0.95cm3/g以上である、請求項13から15のいずれか一項に記載の一次電池用の正極。
- 前記カーボンナノチューブは、25℃の温度および20kNの圧力で体積抵抗率が0.0187Ω・cm以下である、請求項13から16のいずれか一項に記載の一次電池用の正極。
- 前記カーボンナノチューブは、比表面積が200〜300m2/gである、請求項13から17のいずれか一項に記載の一次電池用の正極。
- 請求項13から18のいずれか一項に記載の一次電池用の正極を含む、一次電池。
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